The kinetics of reductive leaching of manganese from a low-grade manganese oxide ore were studied using cellulose as reductant in dilute sulfuric acid medium.It was found that when the stirring speed was higher than 2...The kinetics of reductive leaching of manganese from a low-grade manganese oxide ore were studied using cellulose as reductant in dilute sulfuric acid medium.It was found that when the stirring speed was higher than 200 r/min,the effect of gas film diffusion on manganese extraction efficiency could be neglected,and the kinetic behavior was investigated under the condition of elimination of external diffusion influence on the leaching process.Effects of leaching temperature,mass ratio of cellulose and ore,and the sulfuric acid concentration on manganese extraction efficiency were discussed.The kinetic data were analyzed based on the shrinking core model,which indicated that the leaching process was dominated by both ash layer diffusion and chemical reaction at the initial stage,with the progress of leaching reaction,the rate-controlling step switched to the ash layer diffusion.It was also concluded that the sulfuric acid concentration had the most significant influence on the leaching rate,the reaction orders with respect to the sulfuric acid concentration were 2.102 in the first 60 min,and 3.642 in the later 90 min,while the reaction orders for mass ratio of cellulose and ore were 0.660 and 0.724,respectively.An Arrhenius relationship was used to relate the temperature to the rate of leaching,from which apparent activation energies were calculated to be 46.487 kJ/mol and 62.290 kJ/mol at the two stages,respectively.Finally,the overall leaching rate equations for the manganese dissolution reaction with cellulose in sulphuric acid solution were developed.The morphological changes and mineralogical forms of the ore before and after the chemical treatment were discussed with the support of SEM and XRD analyses.展开更多
ZnO：La3＋,Li＋ nanoparticles were successfully prepared by co-precipitation, citric acid-assisted co-precipitation, co-precipitation combined solid-state reaction and thermal decomposition method. X-ray diffraction ...ZnO：La3＋,Li＋ nanoparticles were successfully prepared by co-precipitation, citric acid-assisted co-precipitation, co-precipitation combined solid-state reaction and thermal decomposition method. X-ray diffraction （XRD）, scanning electron microscopy （SEM） and luminescence spectrophotometry were employed to characterize the crystal phases, particle sizes and luminescence properties of the as-prepared nanopowders. The results indicate that all the prepared samples crystallize in a hexagonal wurtzite structure. The ZnO：La3＋,Li＋ prepared by citric acid-assisted co-precipitation method has a particle size of about 80 nm, which is the smallest among all the samples. Fluorescence （FL） spectra of all samples exhibit three typical emissions： a violet one centered at around 400 nm, blue around 450 nm and 466 rim, and weak green near 520 nm. But the samples prepared by co-precipitation method show a strong and wide green light emission located at about 500 nm. The ZnO：La3＋,Li＋ nanoparticles synthesized by the co-precipitation method demonstrate relatively the strongest emission intensity.展开更多
A novel cloud-point extraction （CPE） was successfully used in preconcentration of biphenol A （BPA） from aqueous solutions. Majority of BPA is extracted into the surfactant-rich phase. The parameters affecting the ...A novel cloud-point extraction （CPE） was successfully used in preconcentration of biphenol A （BPA） from aqueous solutions. Majority of BPA is extracted into the surfactant-rich phase. The parameters affecting the CPE such as concentration of surfactant and electrolyte, equilibration temperature and time and pH of sample solution were investigated. The samples were analyzed by high-performance liquid chromatography with ultraviolet detection. Under the optimized conditions, preconcentration of 10 mL sample gives a preconcentration factor of 11. The limit of detection （LOD） and limit of quantification （LOQ） are 0.1 μg/L and 0.33 μg/L, respectively. The linear range of the proposed method is 0.2-20 μg/L with correlation coefficients greater than 0.998 7 and the spiking recove6es are 97.96%-100.42%. The interference factor was tested and the extraction mechanism was also investigated. Thus, the developed CPE has proven to be an efficient, green, rapid and inexpensive approach for extraction and preconcentration of BPA from water samples.展开更多
The separation of rhenium from molybdenum in aqueous solution has always been a problem in hydrometallurgy. The separation of rhenium from the electro-oxidation leachate of molybdenite and its mechanism were investiga...The separation of rhenium from molybdenum in aqueous solution has always been a problem in hydrometallurgy. The separation of rhenium from the electro-oxidation leachate of molybdenite and its mechanism were investigated. The results show that pH of the leachate significantly affects adsorption rate compared with other experimental parameters. When temperature is 30℃, pH=8, and adsorbing time is 1 h, adsorption rates of rhenium and molybdenum are 93.46% and 3.57%, respectively, and separation factor of D301 resin for rhenium and molybdenum is 169.56. In addition, the separation factor is higher when the initial molybdenum concentration in model solution is increased. The saturated adsorption capacity of D301 resin for molybdenum and rhenium calculated based on simulated results are 4.263 3 mmol/g and 4.235 5 mmol/g, respectively. D301 resin is an effective separation material of rhenium from electric-oxidation leachate of molybdenite. The adsorption kinetics results also show that the adsorption of rhenium is easier than that of molybdenum, and the adsorption process of D301 for rhenium and molybdenum may be controlled by liquid film diffusion.展开更多
The recovery of iron from iron sinking slag and lead smelter slag was investigated by desulfurization-reduction bath smelting. The effects of lead smelter slag(LSS) to iron sinking slag(ISS) mass ratio and temperature...The recovery of iron from iron sinking slag and lead smelter slag was investigated by desulfurization-reduction bath smelting. The effects of lead smelter slag(LSS) to iron sinking slag(ISS) mass ratio and temperature were investigated in desulfurization experiments. The X-ray diffraction(XRD) and X-ray fluorescence(XRF) analyses show that the optimum conditions are LSS:ISS of 3:7 and temperature of 1350°C. The composition of desulfurization products is mainly Zn Fe2O4, and the desulfurization rate of 99.66% is obtained under optimum conditions. The thermogravimetric(TG) and differential scanning calorimeter(DSC) analyses demonstrate that reductant is necessary for decomposition and reduction of zinc ferrite in desulfurization product. The effects of reductant, temperature and feeding modes on iron enrichment were investigated in reduction experiments. The scanning electron microscope(SEM) and energy dispersive spectrometer(EDS) determination show that the iron content of reduction product is up to 99.36% under optimum conditions of coke as reductant, reduction temperature of 1450°C and the feeding mode of premixing.展开更多
The production of environmental friendly emulsion paint is of great significance. Vacuum steam stripping of methyl isobutyl ketone （MIBK） and methyl ethyl ketone （MEK） from cathodic electrophoretic emulsion was st...The production of environmental friendly emulsion paint is of great significance. Vacuum steam stripping of methyl isobutyl ketone （MIBK） and methyl ethyl ketone （MEK） from cathodic electrophoretic emulsion was studied. The effects of mass ratio of vapor to feed （V/F）, vacuum degree and feed temperature on removal rate of MIBK and MEK, emulsion size and solid volume fraction of the emulsion were investigated, and the removal of MIBK and MEK from cathodic electrophoretic emulsion by vacuum desorption was also studied. The results show that removal rates of both MIBK and MEK increase with the increase of V/F, vacuum degree and feed temperature. Removal rates of MIBK and MEK are 98.3% and 93.6%, respectively, at the operating condition V/F of 0.7, feed temperature of 27℃ and vacuum degree of 90 kPa. The emulsion size of cathodic electrophoretic emulsion increases slightly with feed temperature when temperature is below 42 ℃, and increases rapidly with feed temperature when temperature is above 42℃. Solid volume fraction increases by 10% as vacuum degree increases from 0 to 90 kPa at V/F of 0.7 and feed temperature of 27 ℃. Compared with vacuum desorption, vacuum steam stripping can get a higher removal rate of MIBK and MEK under the same feed flow, vacuum degree and feed temperature.展开更多
The mathematical topological rule was applied to plot the predominance area diagram.Based on the analysis of the mutually conjugated,only two diagrams were the best topological embryonic graphs to build the predominan...The mathematical topological rule was applied to plot the predominance area diagram.Based on the analysis of the mutually conjugated,only two diagrams were the best topological embryonic graphs to build the predominance area diagram of Me-S-O system.Combined with topological rules and thermodynamic calculation,four relation-diagrams were denoted asαandβstable and unstable plane-topological diagrams,which were plotted for the Pb-S-O system and Zn-S-O system.The results show thatβstable plane-topological diagram of Pb-S-O system andαstable one of Zn-S-O system are in accordance with the traditional predominance area diagram,which indicates that it is feasible to plot the predominance area diagram based on mathematical topological rules.Meanwhile,αunstable plane-topological diagram of Pb-S-O system can elucidate the phenomenon that metallic lead exists in higher oxygen and sulfur pressure area in modern bath smelting furnace.The mathematical topological rules broaden the application scope of the predominance area diagram and enrich the practice of its plotting.展开更多
One-pot synthesis of cyclic aldol tetramer and α, β-unsaturated aldol from C3-C8 linear aldehydes using phase-transfer catalyst（PTC）, quaternary ammonium, combined with sodium hydroxide as catalysts was investigat...One-pot synthesis of cyclic aldol tetramer and α, β-unsaturated aldol from C3-C8 linear aldehydes using phase-transfer catalyst（PTC）, quaternary ammonium, combined with sodium hydroxide as catalysts was investigated. Butanal was subjected for detail investigations to study the effect of parameters. It was found that the selectivity of cyclic aldol tetramer depends greatly on the operating conditions of the reaction, especially the PTC/butanal molar ratio. The average selectivity of 2-hydroxy-6-propyl-l, 3, 5-triethyl-3-cyclohexene-1-carboxaldehyde（HPTECHCA） was 54.41% using tetrabutylammonium chloride combined with 14%（mass fraction） Na OH as catalysts at 60 ℃for 2 h with a PTC-to-butanal molar ratio of 0.09：1. Pentanal was more likely to generate cyclic aldol tetramer compared with other aldehydes under the optimum experimental conditions. Recovery of the PTC through water washing followed by adding enough sodium hydroxide from the washings was also demonstrated.展开更多
Using Schiff base as a phase transfer catalyst, ethoxycarbonyl isothiocyanate was synthesized by reacting ethyl chloroformate with sodium thiocyanate. In order to get the best synthetic technology, an orthogonal test ...Using Schiff base as a phase transfer catalyst, ethoxycarbonyl isothiocyanate was synthesized by reacting ethyl chloroformate with sodium thiocyanate. In order to get the best synthetic technology, an orthogonal test （L9（34）） was applied. The results show that reaction temperature, reaction time, content of catalyst and molar ratio of sodium thiocyanate to ethyl chloroformate are the main factors influencing the yield. The four factors chosen for the present investigation are based on the results of a single-factor test. The optimum synthetic technology is determined as follows： reaction temperature 35 ℃, reaction time 3 h, the content of catalyst （molar fraction based on ethyl chloroformate） 1.5% and molar ratio of sodium thiocyanate to ethyl chloroformate 1.1. Under the optimized synthetic technology, the experimental yield reaches 96.8%.展开更多
The chemical nature of the interaction of starch and dodecylamine （DDA）, which generally act as depressant and collector, respectively, in the reverse flotation of bauxite, was investigated using starch-iodine tests...The chemical nature of the interaction of starch and dodecylamine （DDA）, which generally act as depressant and collector, respectively, in the reverse flotation of bauxite, was investigated using starch-iodine tests. The results obtained from the blue-value measurements for starch＋DDA＋iodine system indicate the formation of the inclusion complex for amylose-DDA system at low DDA concentration （〈2 retool/L）. However, it is less likely for amylopectin-DDA system with short helix. UV-Vis spectra of starch-iodine complexes show that each helix of amylose can accommodate two DDA molecules locating separately at its two ends, and in the helical cavity there is room available for the upcoming iodine. When concentrated DDA is tested, amylose-DDA system exhibits no characteristic starch-iodine color, owing to the presence of a compact coating of DDA molecules on starch via hydroxyl/amine hydrogen bonding. ^1H NMR spectroscopy and surface tension determination help to clarify the interaction mechanism of amylose with DDA.展开更多
基金Project(2010FJ1011)supported by the Major Project of Science and Technology of Hunan Province,China
文摘The kinetics of reductive leaching of manganese from a low-grade manganese oxide ore were studied using cellulose as reductant in dilute sulfuric acid medium.It was found that when the stirring speed was higher than 200 r/min,the effect of gas film diffusion on manganese extraction efficiency could be neglected,and the kinetic behavior was investigated under the condition of elimination of external diffusion influence on the leaching process.Effects of leaching temperature,mass ratio of cellulose and ore,and the sulfuric acid concentration on manganese extraction efficiency were discussed.The kinetic data were analyzed based on the shrinking core model,which indicated that the leaching process was dominated by both ash layer diffusion and chemical reaction at the initial stage,with the progress of leaching reaction,the rate-controlling step switched to the ash layer diffusion.It was also concluded that the sulfuric acid concentration had the most significant influence on the leaching rate,the reaction orders with respect to the sulfuric acid concentration were 2.102 in the first 60 min,and 3.642 in the later 90 min,while the reaction orders for mass ratio of cellulose and ore were 0.660 and 0.724,respectively.An Arrhenius relationship was used to relate the temperature to the rate of leaching,from which apparent activation energies were calculated to be 46.487 kJ/mol and 62.290 kJ/mol at the two stages,respectively.Finally,the overall leaching rate equations for the manganese dissolution reaction with cellulose in sulphuric acid solution were developed.The morphological changes and mineralogical forms of the ore before and after the chemical treatment were discussed with the support of SEM and XRD analyses.
基金Project(50972166) supported by the National Natural Science Foundation of China
文摘ZnO：La3＋,Li＋ nanoparticles were successfully prepared by co-precipitation, citric acid-assisted co-precipitation, co-precipitation combined solid-state reaction and thermal decomposition method. X-ray diffraction （XRD）, scanning electron microscopy （SEM） and luminescence spectrophotometry were employed to characterize the crystal phases, particle sizes and luminescence properties of the as-prepared nanopowders. The results indicate that all the prepared samples crystallize in a hexagonal wurtzite structure. The ZnO：La3＋,Li＋ prepared by citric acid-assisted co-precipitation method has a particle size of about 80 nm, which is the smallest among all the samples. Fluorescence （FL） spectra of all samples exhibit three typical emissions： a violet one centered at around 400 nm, blue around 450 nm and 466 rim, and weak green near 520 nm. But the samples prepared by co-precipitation method show a strong and wide green light emission located at about 500 nm. The ZnO：La3＋,Li＋ nanoparticles synthesized by the co-precipitation method demonstrate relatively the strongest emission intensity.
基金Project(20956001) supported by the National Natural Science Foundation of ChinaProject(CX2011B083) supported by Hunan Provincial Innovation Foundation for Postgraduate, ChinaProject(K1104026-11) supported by Project of Changsha Science and Technology Bureau, China
文摘A novel cloud-point extraction （CPE） was successfully used in preconcentration of biphenol A （BPA） from aqueous solutions. Majority of BPA is extracted into the surfactant-rich phase. The parameters affecting the CPE such as concentration of surfactant and electrolyte, equilibration temperature and time and pH of sample solution were investigated. The samples were analyzed by high-performance liquid chromatography with ultraviolet detection. Under the optimized conditions, preconcentration of 10 mL sample gives a preconcentration factor of 11. The limit of detection （LOD） and limit of quantification （LOQ） are 0.1 μg/L and 0.33 μg/L, respectively. The linear range of the proposed method is 0.2-20 μg/L with correlation coefficients greater than 0.998 7 and the spiking recove6es are 97.96%-100.42%. The interference factor was tested and the extraction mechanism was also investigated. Thus, the developed CPE has proven to be an efficient, green, rapid and inexpensive approach for extraction and preconcentration of BPA from water samples.
基金Foundation item： Project（21106188） supported by the National Natural Science Foundation of China Project（12JJ4013） supported by Htman Provincial Natural Science Foundation of China+2 种基金 Projects（2011M501299, 2012T50709） supported by China Postdoctoral Science Foundation Project（2011QNZT050） supported by the Special Fund from the Central Collegiate Basic Scientific Research Bursary of Central South University, China Project（CSUZC2012038） supported by the Open-End Fund for the Valuable and Precision Instruments of Central South University, China
文摘The separation of rhenium from molybdenum in aqueous solution has always been a problem in hydrometallurgy. The separation of rhenium from the electro-oxidation leachate of molybdenite and its mechanism were investigated. The results show that pH of the leachate significantly affects adsorption rate compared with other experimental parameters. When temperature is 30℃, pH=8, and adsorbing time is 1 h, adsorption rates of rhenium and molybdenum are 93.46% and 3.57%, respectively, and separation factor of D301 resin for rhenium and molybdenum is 169.56. In addition, the separation factor is higher when the initial molybdenum concentration in model solution is increased. The saturated adsorption capacity of D301 resin for molybdenum and rhenium calculated based on simulated results are 4.263 3 mmol/g and 4.235 5 mmol/g, respectively. D301 resin is an effective separation material of rhenium from electric-oxidation leachate of molybdenite. The adsorption kinetics results also show that the adsorption of rhenium is easier than that of molybdenum, and the adsorption process of D301 for rhenium and molybdenum may be controlled by liquid film diffusion.
基金Project(2011AA061003)supported by the National High Technology Research and Development Program of China
文摘The recovery of iron from iron sinking slag and lead smelter slag was investigated by desulfurization-reduction bath smelting. The effects of lead smelter slag(LSS) to iron sinking slag(ISS) mass ratio and temperature were investigated in desulfurization experiments. The X-ray diffraction(XRD) and X-ray fluorescence(XRF) analyses show that the optimum conditions are LSS:ISS of 3:7 and temperature of 1350°C. The composition of desulfurization products is mainly Zn Fe2O4, and the desulfurization rate of 99.66% is obtained under optimum conditions. The thermogravimetric(TG) and differential scanning calorimeter(DSC) analyses demonstrate that reductant is necessary for decomposition and reduction of zinc ferrite in desulfurization product. The effects of reductant, temperature and feeding modes on iron enrichment were investigated in reduction experiments. The scanning electron microscope(SEM) and energy dispersive spectrometer(EDS) determination show that the iron content of reduction product is up to 99.36% under optimum conditions of coke as reductant, reduction temperature of 1450°C and the feeding mode of premixing.
基金Project(21176264)supported by the National Natural Science Foundation of ChinaProject(ZL110414)supported by the Undergraduate Free Exploration Innovation Foundation of Central South University,China
文摘The production of environmental friendly emulsion paint is of great significance. Vacuum steam stripping of methyl isobutyl ketone （MIBK） and methyl ethyl ketone （MEK） from cathodic electrophoretic emulsion was studied. The effects of mass ratio of vapor to feed （V/F）, vacuum degree and feed temperature on removal rate of MIBK and MEK, emulsion size and solid volume fraction of the emulsion were investigated, and the removal of MIBK and MEK from cathodic electrophoretic emulsion by vacuum desorption was also studied. The results show that removal rates of both MIBK and MEK increase with the increase of V/F, vacuum degree and feed temperature. Removal rates of MIBK and MEK are 98.3% and 93.6%, respectively, at the operating condition V/F of 0.7, feed temperature of 27℃ and vacuum degree of 90 kPa. The emulsion size of cathodic electrophoretic emulsion increases slightly with feed temperature when temperature is below 42 ℃, and increases rapidly with feed temperature when temperature is above 42℃. Solid volume fraction increases by 10% as vacuum degree increases from 0 to 90 kPa at V/F of 0.7 and feed temperature of 27 ℃. Compared with vacuum desorption, vacuum steam stripping can get a higher removal rate of MIBK and MEK under the same feed flow, vacuum degree and feed temperature.
基金Project(2011AA061003) supported by the High-Tech Research and Development Program of China
文摘The mathematical topological rule was applied to plot the predominance area diagram.Based on the analysis of the mutually conjugated,only two diagrams were the best topological embryonic graphs to build the predominance area diagram of Me-S-O system.Combined with topological rules and thermodynamic calculation,four relation-diagrams were denoted asαandβstable and unstable plane-topological diagrams,which were plotted for the Pb-S-O system and Zn-S-O system.The results show thatβstable plane-topological diagram of Pb-S-O system andαstable one of Zn-S-O system are in accordance with the traditional predominance area diagram,which indicates that it is feasible to plot the predominance area diagram based on mathematical topological rules.Meanwhile,αunstable plane-topological diagram of Pb-S-O system can elucidate the phenomenon that metallic lead exists in higher oxygen and sulfur pressure area in modern bath smelting furnace.The mathematical topological rules broaden the application scope of the predominance area diagram and enrich the practice of its plotting.
基金Project(2013AA064102)supported by the National High-Tech Research Program of ChinaProject(11JJ6014)supported by the Hunan Provincial Natural Science Foundation of China
文摘One-pot synthesis of cyclic aldol tetramer and α, β-unsaturated aldol from C3-C8 linear aldehydes using phase-transfer catalyst（PTC）, quaternary ammonium, combined with sodium hydroxide as catalysts was investigated. Butanal was subjected for detail investigations to study the effect of parameters. It was found that the selectivity of cyclic aldol tetramer depends greatly on the operating conditions of the reaction, especially the PTC/butanal molar ratio. The average selectivity of 2-hydroxy-6-propyl-l, 3, 5-triethyl-3-cyclohexene-1-carboxaldehyde（HPTECHCA） was 54.41% using tetrabutylammonium chloride combined with 14%（mass fraction） Na OH as catalysts at 60 ℃for 2 h with a PTC-to-butanal molar ratio of 0.09：1. Pentanal was more likely to generate cyclic aldol tetramer compared with other aldehydes under the optimum experimental conditions. Recovery of the PTC through water washing followed by adding enough sodium hydroxide from the washings was also demonstrated.
基金Project(2007AA06Z122) supported by the National High Technology Research and Development Program of ChinaProject(20110491267) supported by the Postdoctoral Science Foundation of ChinaProject(74341015502) supported by Postdoctoral Fund of Central South University,China
文摘Using Schiff base as a phase transfer catalyst, ethoxycarbonyl isothiocyanate was synthesized by reacting ethyl chloroformate with sodium thiocyanate. In order to get the best synthetic technology, an orthogonal test （L9（34）） was applied. The results show that reaction temperature, reaction time, content of catalyst and molar ratio of sodium thiocyanate to ethyl chloroformate are the main factors influencing the yield. The four factors chosen for the present investigation are based on the results of a single-factor test. The optimum synthetic technology is determined as follows： reaction temperature 35 ℃, reaction time 3 h, the content of catalyst （molar fraction based on ethyl chloroformate） 1.5% and molar ratio of sodium thiocyanate to ethyl chloroformate 1.1. Under the optimized synthetic technology, the experimental yield reaches 96.8%.
基金Project(50804055) supported by the National Natural Science Foundation of China
文摘The chemical nature of the interaction of starch and dodecylamine （DDA）, which generally act as depressant and collector, respectively, in the reverse flotation of bauxite, was investigated using starch-iodine tests. The results obtained from the blue-value measurements for starch＋DDA＋iodine system indicate the formation of the inclusion complex for amylose-DDA system at low DDA concentration （〈2 retool/L）. However, it is less likely for amylopectin-DDA system with short helix. UV-Vis spectra of starch-iodine complexes show that each helix of amylose can accommodate two DDA molecules locating separately at its two ends, and in the helical cavity there is room available for the upcoming iodine. When concentrated DDA is tested, amylose-DDA system exhibits no characteristic starch-iodine color, owing to the presence of a compact coating of DDA molecules on starch via hydroxyl/amine hydrogen bonding. ^1H NMR spectroscopy and surface tension determination help to clarify the interaction mechanism of amylose with DDA.
